Apparatus for dezincing lead



Oct. 25, 1932. J. o. BETTERTON APPARATUS FOR DEZINCING LEAD Original Filed May '7, 1926 2 Sheets-Sheet 1 BY WW-M ATTORNEY Ott. 25, 1932v 1 BETTERTQN 1,884,533

APPARATUS FOR DEZINCING LEAD Original Filed May 7, 1926 2 Sheets-Sheet 2 INVENTOR 0% BY Mam -ATTORNEY name use, 1932 p UNITED srarasraraur orrlcs JESSE OATKAN BETTEBTON, OI OIAHA KA, ASSIGNOA TO AMERICAN SMELTING Application fled Kay 7, 1998, Serlal Io. 107,885. Renewed February 27, 1929.

, This invention relates to apparatus for refining metals, and, more paratus for 'de'zincing lea 7 According to the invention, a metal having as an impurity metals electropositive to said metal, is subjected in'a novel manner to the action of a aseous or other reagent, which unites with t c more electropositive metal to remove the same. as a slag or dross.

The process makes use of the fact that a reagent such as chlorine has a greater aflinity for certain metals, such as metallic zinc, than for other metals, such as metallic-lead, when the metals are together in a molten state. For example, lead with zinc as an Impurity therein may be the bullion resulting from any-metallurgical process. The lead ulhon may be that result-mg from the Parkes processafter the silver has been removed'by th'e use of zinc. In lead resulting from the Parkes process the amount of zinc remaining in the 'lead may be approximately 0.55 'percent, or 11 pounds of zinc per ton of lead. In order to remove the zinc from the lead approximately 1.085 pounds of chlorine are re-' quired theoretically for every pound of zinc, and therefore for every 100 tons of lead there would be required approximately 1193 pounds of chlorine.

According to the invention, practically the entire montage of zinc is removed by the use of ale more than the theoretical amount of chlorine necessary to remove the zinc.

This results in great economy of chlorine as well as great. sa

ety and comfort in refining,

because of the" fact thatrgractically no unused chlorine escapes. e reaction of the chlorine with the zinc produces considerable heat. The zinc chloride formed by the reaction, and particularly the chlorine, are very corrosive at the temperature which is produc'ed by the reaction, and are therefore very.

destructive to metal with which they come in contact. According'to the invention, how

ever, the process is so carried out that the chlorine and zinc. chloride have no serious efiect on the metal of the apparatus which is employed to carry outthe process.

' According to the invention, a portion of the bath ofmolten lead containing zinc as an imgartlcularly, to ap- 'AND DEFINING OOIPANY, 0] NEW YORK, N. Y, A CORPORATION OF JERSEY APPARATUS FOR DEZINCING P i y is continuously removed and chlorin -r.

is added to such portion, which is then returned to the bath below its surface a sufficient distance to fermita skim or dross of zinc chloride to orm on the surface. .The

process is'carried on at a relatively low tem- ,perature-above the melting point of the lead and at a temperature which will cause the molten dross of zinc chloride to partially solidlfy on the surface of the bath, thereby forming a seal which tends to prevent the escape of chlorinefrom the bath. The chlorine is supplied in amounts proportional to the quantities of zinc or other impurities in the bath, and'under proper conditions to revent injury to the walls of the reaction c amber and Thus if any lead combines with the chlorineto form leadchloride, the zinc will immedi ately combine with the lead chloride to form zinc chloride and pure lead, provided suflicient zinc is still present in the bath. I

The first skimmings of the kettle will be practically pure zinc chloride. The later ings, as the amount of zinc in the bath is decreased, however, may contain some leadv chloride in addition to the zinc chloride. This lead chloride may be skimmed OE and kept separate'and may be used to treat subsequent charges of lead bullion containing zinc prior to treatment with chlorine gas.

Various other features of the invention will be obvious from the following particulardebe considered as two scription of the process and from the particular description of forms of apparatus for carrying out the process, or from an inspection of the accompanying drawings; and the invention also consists in certain new and novel'steps of the process and new and novel features of the construction, and combinatrates suita le apparatus for carrying out the nel -1rons. 4 extending across process:

Fig. 1 is an elevational view partly in section a showing one form of apparatus for carrying out the improved process;

Fig. 2 is a detail taken'on the line 22 of Fig. 1;

Fi 3 is an elevational view partly in section s owing an improved form of apparatus for carrying out the invention; and

Fig. 4 is a plan view of the apparatus shown in Fig. 3.

In the fol owing description and in the claims parts will be identified by specific names for convenience, but they are intended to be as generic in their application to similar parts as the artwill permit.

, Referring now to Figs. 1 and 2, the lead kettle 1 may be filled with molten lead containing zinc to the heightindicated by the line 14. Supported by the top rim of the kettle is a unit comprising a motor,,2 and pump 3, the motor being supported by chanthe kettle and resting upon the rim thereof. The pump is suspended from the motor and is located near the bottom of the kettle. The unit may be provided with a link 5 by means of which the unit may be carried about the plant,. as

from this kettle to another kettle.

Supported also on the rim of the kettle 1 is a reaction cylinder 6 which may comprise a short length of pipe, ,the bottom of the cylinder being closed and having a discharge which ma ipe 7 connected thereto which extends down Beneath the surface of the bath a suitable distance. If desired this discharge pipe may not extend below the surface of the molten lead, but the dischar e opening may be sealed inst escape of c orine by extending into area of the dischar e o nmg that a ody of molten lead (0 en stantial depth) is maintained in the bottom of the chamber to prevent leakage of the gas. I may even submerge the entire reaction chamber beneath the surface of the molten lead. The reaction cylinder 6 may be supported by two I-beams .8 extendingacross the kettle, the I-beams having secured at their lower flanges transverse members 9 on which the reaction cylinder rests. The top of the reaction cyhnder .may be provided with a flange 10 to be secured a cylinder head 11. may be connected from the discharge and of the pump 3 to the top of the head of the reaction cylinder, this pipe having a tie j 7 union 16 for a purpose hereinafter descri d.

If desired, a four-way union 17 may be connected to the head of the reaction cylinder by a short nipple 13 as shown in Fig. 2,

A connecting p'ipe Located conveniently near the kettle may and the reaction cylinder.

toa

be the source of chlorine, which may be in the form of a chlorine tank 18 immersed in a vessel 19 filled with water and kept at an appropriate temperature. Suitable piping 20 may connect the chlorine tank with the reaction cylinder and a valve 21 may be provided for controlling the flow of the chlorine.

If desirable a ring of iron 12 maybe rovided to float on the surface of the bat to provide a restricted area in which the slag may be collected and removed.

It is not always advantageous to have the reaction cylinder and pump and motor unit as separate units. Therefore, in Figs. 3 and 4 the reaction cylinder, motor and pump are provided in a single unit, which may be en plied to or removed from the bullion kett ie as a unit.

Referring now to Figs. 3 and 4, a lead bullion kettle is shown, on which is positioned a reaction cylinder 31, pump 32, motor 33 and gear case 34, all mounted on a frame so that they can be moved from place to place as a single unit. The framework may comprise a transverse I-beam 35 to which may be connected at r' ht angles a pair of spaced, parallel, latera y extending I-beamsi 38 which extend beyond the rim of the kettle. Located between each of the I-beams 35 and 38 and the rim of the kettle may be spacing pieces 39, for taking the wear incidental to placing1 the unit on and removing the unit rom t e several'kettles in the refining plant, and to withstand the heat, thereby protecting the I-beams from heat and wear. A pair of projecting I-beams 40 may be provided extending laterally on the opposite side of the transverse reaction cylinder 31.

Supported on the laterally extending I- beams 38 may be the bed plate of a motor and gear unit, the pump 32 being suspended from the gear case 34 so as to be driven by thefmotor 33. The discharge side of the pump 32 is connected to the to of the reaction cylinder 31, a flanged coup ing 41 being provided in the connecting pipe 42 as in igs. 1 and 2. The reaction cylinder may be provided with a dischar e pipe 43,- as in igs. 1 and 2, which ex'ten beneath the .surface of the bath. It will be understoodthat a chlorine tank with necessary connectin piping and a control valve may be provide to supply the reaction cylinder 31 with the necessary reagent as in Fi s. 1 and .2. An iron ring 44 may be provide if desirable, as in Figs. 1 and 2. The level of the lead bath may be at 45. I

The improved process will be explained ill with reference to the modification shown in Fig. 1 but it will be understood that the process alsomay be practiced with the apparatus shown in Figs. 3 and 4. The motor and pum and also the reaction cylinder may be plac in the, position shown after the kettle 1 has been filled to the level indicated, with molten lead. The parts of the connecting pipe may be connected together by means of the. flanged coupling 16, and the pump may be started and run for a few minutes to circulate the molten lead through the reaction cylinder to clean out any slag which may have adhered thereto from previous charges and also to warm up the cylinder. The pump is then stopped and the chlorine tank is connected to the reaction cylinder, and the chlorine turned on until it bubbles at the surface of the bath. The pump is then started and the chlorine valve opened as far as possible without allowing the gas to esca at the surface of the lead.

ince the reaction of chlorine and zinc produces considerable heat, sufiicient lead bullion must be kept circulating througli the reaction cylinder to prevent the temperature of the reaction cylinder from getting too high. This continuous circulation prevents corrosion of the reaction cylinder by the zinc chloride, and especially the chlorine, and washes the zinc chloride which is formed quickly through the discharge pipe and into the bath, where it floats to the surface in the form of a dross. In general, the cooling of the ap aratus and the rate atwhich the heat is allbwed to generate should be so arranged to give a temperature of about'670 degrees to 750 degrees F., at which temperature the improved process gives good results.

If the temperature is too high, the zinc chloride will volatilize quite appreciably where the lead bath is agitated or disturbed in any manner, as by the stream of lead discharged from the discharge pipe or by skimming ofi the zinc chloride; corrosion of the reaction cylinder by the chlorine and zinc chloride is increased at a relatively high temperature; also at higher temperatures the lead has a greater tendenc to react with the.

chlorine which is undesira le. It is desirable to regulate the temperature to cause the top 'layers of molten zinc chloride slag floating: on the bath to freeze. As the frozen layers are removed by skimming new layers freeze, thereby'sealing the bath and preventing escape of the ch orine.

On the other hand, ifthe temperature is too low it becomes difficult to start the ump. Otherwise the process could be carri on at a temperature near the melting point of the bath.

Preferably the chlorine should be delivered to the reaction cylinder under a slight pressure. For example, the chlorine tank was placed in water having a temperature of to degrees F. This provided the pro r conditions to cause the chlorine to be f to the reaction cylinder at the desired rate of 200 to 250 pounds per hour, while the molten lead was circulated through the reaction chamber at the rate of'225 tons per hour.

When chlorine was fed at theabove rate and the lead was pumped through the reaction 0 linder in the particular manner and with t e part1cular apparatus above stated,

the level of the lead in the reaction cylinder was, for example, about 3 to 4 inches above the top of the discharge pipe. In general, the rate of flow of the lead and the other conditions should be arranged to allow a sufiicient space within the reaction cylinder to be filled with chlorine gas, through which the lead bullion may be pumped in a stream, to insure thorough mixing of the chlorine with the impure lead.-

If chlorine is fed at too eat a rate to the reaction cylinder, it will e forcedout the discharge pipe and may bubble throu h at the sur ace of the bath. On the other and, if the chlorine is fed too slowly, the progress of dezincing is slowed down but no other detrimental effects result.

It will be evident from the foregoing that, in normal operation, for any given size of reaction cylmder and discharge pipe, the rate of passing the lead through the reaction cylinder may be varied over a definite r e. The rate of feeding chlorine may be varied both in relation to the speed of passing lead through the reaction cylinder and the zinc contents of the lead at the particular time. In order to maintain a maximum rate of feeding chlorine, advantage should be taken of increased speed of pumping as the zinc content decreases.

It has been found satisfactory to skim the dross or slag of zinc chloride from the top of the bath in the kettle while running, since the top of the layer reforms and freezes so rapidly that no appreciable loss 'of chlorine results; After practically all of the zinc is removed from the bath, a white slag of lead chloride will appear. When this ha pens, the pump is stopped and when the c orine bubbles through to the surface of the bath, the chlorine is shut off and the chlorine ipe disconnected. The pump is then starte for a minute or so to insure that the reaction cylinder is thoroughly cleaned out. The kettle may be then skimmed clean. It is necessary to disconnect the chlorine pipe as above ing displaced by lead from the pump.

Otherwise, if the chlorine pipe was not disconnected, the reaction cylinder would remain filled with chlorine and a slag would p portedby formed at the surface of the lead in the connecting pipe-and discharge pipe. This would prevent startin later, and would subject the reaction cylin er to corrosion from chlorine and zinc chloride when the apparatus Was out of use. p

v The final slag on the surface of the bullion remains liquid much longer than previous slags, and as it does not freeze fast enough for-skimming clean, and as it is too thin forladling, considerable time may be lost in waiting for the slag to freeze if some remedy is not provided. In order to overcome this difliculty, a button of pure cold lead may be placed in the kettle after the apparatus is removed skimming.

By the improved process it is possible to refine lead containing zinc to such an extent that the refined product will contain less than 0.003 percent zinc. There is practically no loss of lead at the low temperatures at which the process isoperated, since the selective action of the chlorine upon the zinc $5 is more marked at low temperatures. The

zinc chloride is relatively pure and is in commercial form without subsequent refining or treatment. v

The material being treated is maintained in a relatively large pool in a receptacle having a large radiating surface whereby a relatively low temperature can be maintained notwithstandin the heat of the re-action which occurs. onsequentl there is no excessive -agitation of the bat in the receptacle so that a la er of dross may readily form on top of the hath, which, in the case of zinc chloride,

rapidly cools at atmospheric temperatures,

I thereby forming a seal that prevents escape of chlorine which might otherwise occur.

Although a description has been given for pu of illustration of particular forms of t e ap aratus and of certain details of a method 0? racticing the invention,'it is obvious that t e invention is not limited to this articular apparatus and method, but is road enough to include an apparatus of any size and any method, so ong as the broad teaching of the invention is followed. Furthermore, the invention is not limited to the purification of lead containing zinc by means of gaseous chlorine, but is broad enough to to cool the lead bath sufliciently for with said detachable head, means con-" nected to the detachable head for supplyin a reactive gas to the reaction cylin er, a discharge pipe depending from the base of the reaction cylinder and adapted to be immersed in the bath to a substantial extent. I

In testimony whereof I have hereunto set my hand.

JESSE OATMAN BETTERTON.

include the purification of any material or metal by any kind of a gaseous or other reagent.

Having claim:

Apparatus for the purification of metals, comprisin a framework adapted to be supe rim of a kettle containing a bath of molten metal, a motor su ported by said framework, a pump depen ing from 'said framework and driven by said motor, said pump being adapted to be immersed below the surface ofthe bath, a reaction cylinder thus described my invention, I 

